GC Analysis of Aldehydes (PFBOA Derivatives) in Beer on SLB®-5ms after SPME using a 65 μm PDMS/DVB Fiber

GC Analysis of Aldehydes (PFBOA Derivatives) in Beer on SLB®-5ms after SPME using a 65 μm PDMS/DVB Fiber


sample preparation derivatization procedure: Add 100 µL of PFBOA solution (6 g/L) to 10 mL of deionized water in a 20 mL glass vial and seal. (Insert the PDMS/DVB SPME fiber in the headspace of the PFBOA solution for 10 min at 50 °C.)
sample/matrix 10 mL of degassed beer, 3.5 gm sodium chloride in 20 mL vial
desorption process 0.10 min, 250 °C
extraction 60 min, headspace, 50 °C, agitation (5 min on, 30 min off)
SPME fiber PDMS-DVB, 23 guage, 65 µm, Auto, Pk/3 (57345-U)
column SLB-5ms, 30 m x 0.25 mm I.D., 0.50 µm (28473-U)
oven 40 °C, 7 °C/min to 250 °C (14 min)
carrier gas helium, 1.1 mL/min
sample Beer
injection splitless
liner 0.75 mm I.D. SPME liner
inj. temp. 250 °C
detector MSD, SIM
MSD interface 275 °C


Analysis Note The formation of aldehydes is a major contributor to the deterioration in flavor or "staling" of beer upon storage. Research indicates that the source of these aldehydes is the type of malt used and quality of the wort produced during the brewing process. This application illustrates the use of SPME to extract aldehydes from beer, followed by on-fiber derivatization with 0-(2,3,4,5,6- pentafluorobenzyl)hydroxylamine hydrochloride (PFBOA). The aldehydes are then analyzed by GC/MS-SIM as their corresponding PFBOA derivatives. The aldehydes exist as geometric isomers, resulting in two derivatives for each. In the case of several of the analytes, these two derivatives were resolved chromatographically.
Categories Analytical Chromatography, Food & Beverage Analysis, SPME Applications, GC Applications, Foods, Flavors & Fragrances, Beverage Testing, Aldehydes, Beer, Wine, and Spirits, Beer
Featured Industry Food and Beverages
Legal Information SLB is a registered trademark of Sigma-Aldrich Co. LLC
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